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In the era of the energy transition, the development of sustainable, high-performance, and multifunctional catalysts that adapt to complex catalytic processes is essential. Here, we report shapeshifting bimetallic iron–nickel catalysts developed via an exsolution strategy for carbon dioxide–mediated ethane conversion. By controlling the reduction temperature of a perovskite host, either alloyed iron–nickel nanoparticles or oxide–alloy core–shell nanoparticles are selectively formed. Oxidative regeneration of the perovskite enables reversible interconversion between these distinct nanostructures within the same parent material. As a result, the catalyst exhibits switchable selectivity between ethane dry reforming and carbon dioxide–assisted oxidative dehydrogenation while maintaining high stability. Repeated redox cycling confirms that the structural transformation and catalytic performance are largely reversible. These results demonstrate that exsolution provides a robust platform for designing regenerable catalysts with deliberately tunable and switchable catalytic states.
Single-particle small-angle X-ray scattering (SP-SAXS) at X-ray free electron lasers (XFELs) enables quantitative analysis of morphological heterogeneity that is fundamentally inaccessible to ensemble-averaged in situ techniques. By recording diffraction snapshots from isolated particles, SP-SAXS resolves low-contrast, less abundant, or transient species within heterogeneous particle populations that would otherwise remain hidden to conventional X-ray techniques. We demonstrate this unique capability by investigating the solvothermal formation of CoO nanocrystal assemblies from a Co(acac)3 precursor in benzyl alcohol. The single-particle data revealed amorphous, uniform-density Co(acac)2 spheres as transient intermediates that directly crystallize into cavernous CoO nanocrystal assemblies, explaining why CoO forms as hierarchical aggregates rather than as isolated nanocrystals. These results establish SP-SAXS as a uniquely powerful framework for uncovering nonclassical nanoparticle formation pathways hidden in ensemble measurements.
